CN101270545B - Degumming flame-proof process technique for Han fibrilia - Google Patents
Degumming flame-proof process technique for Han fibrilia Download PDFInfo
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Abstract
The invention discloses a Chinese bast fiber degumming flame retardant treatment technique. The technique carries out ultraviolet radiation, quencher and heating treatments after hot water bath, pre-pickling and pre-chlorination treatments; then carries out alkali oxygen-machine combined degumming treatment and finally carries out flame retardant treatment for twice repeatedly. The surface of the Chinese bast fiber treated by the technique has excellent degumming effect and is better than degumming with a normal alkali oxygen method and a mechanical method; the flame retardant effect is better than the effect of flame retardant post treatment aimed at a Chinese bast fabric and a better white content is obtained; a special blanching working procedure and a flame retardant working procedure are not needed to be arranged in post finishing, thus shortening the flow and saving the cost; the length and the fineness of the fiber are also improved after treatment; less polluting waste water is discharged. The invention is a green and environment protective technical method.
Description
Technical field
The present invention relates to a kind of fire retardant treatment process that comes unstuck at the former flax fibre of Chinese fiber crops (being hemp), particularly on the basis of alkali oxygen-mechanically combining degumming method, be that different phase adds different reagent, and a kind of degumming flame-proof process technique for Han fibrilia that adopts measures such as quenching, heating, thermokalite bath and intensive ultraviolet radiation to carry out.
Background technology
The Degumming method of existing Chinese fiber crops (being hemp) fiber is a lot, its degumming effect respectively has outside the pluses and minuses, also ubiquity following problem: the loose separation of back fiber of coming unstuck, the same very easily burning with other native cellulose fibre, its textiles can not be used in special places such as the high heat of high temperature, also need in the arrangement of back, to carry out special flame-proof treatment and just can reach requirement, after adopting pre-chlorine treatment process that china-hemp fibers is handled as the Jiang Guohua of Hunan Institute Of Engineering, its residual gum content is 3.49%, does not reach the requirement about 2%, and residual lignin is 0.94%, be higher than 0.8%, to spinning post-finishing, especially dyeing is handled adverse effect, and fibre whiteness is lower, very easily burning, also need in the arrangement of back it to be carried out special bleaching or flame-proof treatment, the flow process lengthening is wasted time and energy.The Qu Lijun of University Of Qingdao etc. studied a kind of at china-hemp fibers revolve roll-type physical mechanical Degumming method, but can only effectively dispel in the raw ramie 30% colloid, and fibre whiteness is lower, it is not good to exist flame retardant effect equally, need carry out flame-retardant after-finishing and handle.After the Qu Lijun of University Of Qingdao etc. adopted the short flow process degumming and bleaching of alkaline oxygen bath one-step method new technology that Chinese fiber crops are handled, its ultimate strength was 29.6cN, and residual gum content is 3.82%, be higher than the requirement about 2%, do not reach the requirement that appropriateness is come unstuck, residual lignin is 3.25%, is higher than 0.8%, to spinning post-finishing, especially it is 45.7 that the processing of dyeing has adverse effect, whiteness, still on the low side, though fiber separation is fine, flame retardant effect is the while variation also.
Because china-hemp fibers is a kind of cellulose fibre, the anti-flammability of itself is just poor, and the simple processing of coming unstuck can make fiber become clean more and disperse, this will make more easy firing of fiber, flame retardant effect is variation more, when use in special places such as the high heat of high temperature, also need carry out special flame-retardant after-finishing, this not only makes the technological process lengthening, and the flame retardant effect of the flame-retardant after-finishing flame-retardant after-finishing of Chinese linen (especially to) is not fine, and the color and luster deepening, feel is stiff, the dyefastness variation.At present, flame retarding process about fiber and fabric has had a lot of reports, the research of environment friendly flame retardant and preparation have also had new development, but rare research of flame retarding process and report for Chinese fiber crops (being hemp), also mainly be confined in the arrangement of back, Chinese linen be carried out flame treatment even have, this is because contain the toxic component THC of certain content in the china-hemp fibers, and present stage cultivation and the low toxicity of using or nontoxic Chinese fiber crops kind are also few, add hemp fiber degumming than effects limit such as other flax fibre difficulties the application and the development of china-hemp fibers, this just causes most researchers mainly to focus on the cultivation of low toxicity Chinese fiber crops and the processing of coming unstuck of china-hemp fibers, and is not enough to the flame treatment degree of concern of china-hemp fibers.The report of existing fire retardant treatment process about Chinese linen has: German Saxony textile research R.Bochmann and R.Hubner in " arrangement of hemp Casual Wear and Work Clothes " document, adopt mechanical finishing; chemical finishing and mix finishing technique to pure Chinese fiber crops TWILL CLOTH bleach with flame treatment after; its phosphorus content is 1.56%; no molten drop forms; compare with the textile TWILL CLOTH that is used for this protectiveness Work Clothes; reach same finishing effect; the antiflaming finishing agent that is used for Chinese fiber crops can reduce 25%-30%; saved cost; also reduced the sewage emissions amount; but the limited oxygen index of handling the back fabric only is 29.9; reduce to 29.5 after 5 washings; flame retardant effect is not very desirable; and color and luster deepening; feel is stiff; the dyefastness variation; the more important thing is; this technology is to fabric rather than flame-proof treatment that fiber is carried out; fire retardant mainly covers the surface of fabric; the fire retardant that enters fabric is less; unstable with combining also of fabric, thereby fire-retardant uniformity and washing fastness are bad.
Summary of the invention
The purpose of this invention is to provide a kind of degumming flame-proof process technique for Han fibrilia, have to solve that to exist residual gum content in Chinese retting process higher now, the flame retardant effect variation, the lignin removal effect is undesirable, and whiteness is lower, the stiff and dyeing problem such as not firm of feel, the present invention is in fire retardant treatment process is come unstuck in employing, simultaneously to china-hemp fibers come unstuck, fire-retardant and bleach triple PROCESS FOR TREATMENT, shorten back arrangement flow process, save cost.
The present invention realizes that above-mentioned purpose and the technical scheme that solves the problems of the technologies described above comprise that processed by hot bath, preimpregnation acid treatment, the pre-chlorine of fiber are handled, alkali oxygen-mechanically combining comes unstuck processing, thermokalite is bathed processing, quenching processing and intensive ultraviolet radiation treatment process, be characterized in after pre-chlorine is handled, carry out following steps (in the following steps, the proportioning of fiber and solution is soaks 25 gram fibers in every liter of solution, promptly the concentration of china-hemp fibers in solution is 25g/L):
(1) UV radiation: will soak the china-hemp fibers of 25g/L, the hydrogen peroxide of 10-14g/L, the NaOH of 10-14g/L and the magnesium sulfate MgSO of 3-4g/L
4Mixed solution placed under the ultraviolet light of 280-350nm radiation 30-50 minute;
(2) quenching is freezed to thaw with high temperature: fiber after the radiation and mixed solution are stirred in the lump, and quenching places its taking-up 100 ℃-120 ℃ constant temperature boiling water to thaw fully until ice cube to freezing then;
(3) alkali oxygen-mechanical kiering: in the fiber after thawing, adding the boiling-off auxiliary agent stirs, kiering 150min-200min in 100 ℃-120 ℃ water bath with thermostatic control, and the NaOH, hydrogen peroxide and the magnesium sulfate MgSO that in 20min-30min adding above-mentioned steps (1), configure
4The state of mixed solution before kiering, to carry out mechanical agitation simultaneously, stir speed (S.S.) is 150-200r/min, alr mode be every 20min-30min suitable/stir counterclockwise alternately;
(4) flame-proof treatments: the titanium pigment flame retardant, 18-22g/L silane resin acceptor kh-550, the 2-5g/L anion surfactant that 1. the china-hemp fibers after the kiering are immersed in 140-180g/L
Carry out thermokalite in the mixed solution of the NaOH of H-95 and 10-14g/L and bathe processing, it is 60 ℃-80 ℃ that thermokalite is bathed the temperature of handling, time is 40min-60min, carry out mechanical agitation simultaneously, stir speed (S.S.) is 80-100r/min, alr mode be every 10min-20min suitable/stir counterclockwise alternately; 2. it is radiation 30min-50min under the ultraviolet ray of 280nm-300nm that the china-hemp fibers after thermokalite being bathed places wavelength together with mixed solution; 3. the fiber after the radiation is put into suddenly together with mixed solution and is frozen the case quenching to freezing;
(5) secondary flame-proof treatment: take out the fiber and the mixed solution that freeze and repeat a step;
(6) room temperature is thawed: the fiber after the secondary flame-proof treatment and mixed solution are statically placed in the room-temperature water bath slowly thaw;
(7) fiber after thawing successively carries out operation such as scutching-dehydration-oil supply-de-oiled water-dry/dry etc.
The composition of boiling-off auxiliary agent and content are described in the degumming flame-proof process technique for Han fibrilia of the present invention: waterglass sodium metasilicate (Na
2SiO
3) 0.1-0.3g/L, vulcanized sodium (Na
2S) 1-3g/L, sodium phosphate trimer (Na
5P
3O
10) 1-3g/L, sodium sulfite (Na
2SO
3) 0.7-0.9g/L; Described titanium pigment flame retardant is fire retardant FPK8001 and antiflaming finishing agent SAF8018.
During the technical scheme of the above-mentioned frozen-irradiated auxiliary degumming process for china-hemp fibers of the invention process, its main process characteristics are: (1) is at the pretreatment stage of china-hemp fibers, adopt hot bath, pre-pickling and special pre-chlorine to handle, so not only make fiber loose, remove the part water-solubility impurity, be beneficial to and come unstuck, and make fiber obtain preliminary oxidation bleaching and abundant swollen, the most important thing is to overcome the shortcoming that simple pickling processes makes lignin be difficult to remove; (2) china-hemp fibers is before a kiering, add NaOH, hydrogen peroxide and stabilizing agent magnesium sulfate in advance, and be placed on radiation under the intensive ultraviolet, make its fiber surface gelatinous layer be subjected to etching and destruction, increase and expanded crack, and most of cellulose of oxidation and part lignin, fibre whiteness is increased, the easier dissolving of lignin comes off; (3) fiber after the radiation is put into suddenly together with mixed solution and is frozen the case quenching to freezing, take out then and put into the heating of constant temperature boiling water and thaw, in this process, rapid pucker ﹠ bloat in various degree takes place in fiber and colloid matrix simultaneously, cause its positive and negative drawing power effect that is subjected to vertical and horizontal, make colloid further destroy even come off; When (4) fiber after thawing being carried out the boiling-off of alkali oxygen method together with original mixed solution, add boiling-off additive, and take the circumstances into consideration to replenish the mixed solution of hydrogen peroxide, NaOH and the magnesium sulfate of evaporating loss, simultaneously with suitable/mechanical agitation of replacing counterclockwise, make that china-hemp fibers is easier to come unstuck; (5) when flame-proof treatment, 1. the china-hemp fibers after the kiering is immersed in titanium pigment flame retardant, silane resin acceptor kh-550, anion surfactant
Carry out thermokalite in the mixed solution of H-95 and NaOH and bathe processing, carry out mechanical agitation simultaneously, so not only make the moisture of fiber absorbs abundance, become looser, be beneficial to fire retardant and enter fibrous inside, and can remove the water-solubility impurity of fiber surface, and make the fiber cleaning more that becomes, eliminate the adverse effect of impurity to flame treatment.2. the china-hemp fibers after thermokalite being bathed places radiation under the intensive ultraviolet, make its fiber surface be subjected to etching and destruction, increase and expanded crack, fire retardant is easier to enter inner grafting, and under coupling agent, surfactant and ultraviolet radiation, the graft effect of fire retardant is better; 3. the fiber after the radiation is put into suddenly together with mixed solution and is frozen the case quenching to freezing, rapid contraction in various degree will take place in each position of fiber, change fibrous inner structure, make to enter the fibrous inside fire retardant and be subjected to the squeezing action of vertical and horizontal and adhere to more firmly, graft effect is better; (6) fiber and the mixed solution that freezes repeated above-mentioned steps, carry out the secondary flame-proof treatment, make the percent grafting of fire retardant higher, the grafting fastness is better.(7) fiber after the secondary flame-proof treatment and mixed solution being carried out room temperature slowly thaws.(8) the back fiber that thaws successively carries out operations such as scutching-dehydration-oil supply-de-oiled water-dry/dry.
The Chinese fiber crops that process of the present invention is handled are compared with the Chinese fiber crops that prior art is handled, the present invention is at alkali oxygen--on the basis of mechanically combining degumming method, add different reagent in different phase, and further adopt quenching, heating, the processing method of thermokalite bath and intensive ultraviolet radiation, solved not only that to exist residual gum content in the existing Chinese retting process higher, the lignin removal effect is undesirable and whiteness is lower, the flame retardant effect variation, feel is stiff, problems such as dyefastness variation, and coming unstuck with the Chinese former flax fibre of fiber crops, bleaching and flame treatment are incorporated in the technology to be finished, and has shortened back arrangement flow process, has saved cost.Simultaneously on the basis that has obtained good whiteness and anti-flammability, the ultimate strength of fiber and percentage elongation be controlled at spin within the requirement; The length and the fineness of fiber also are improved, and wearability improves greatly.Its concrete beneficial effect also is:
(1) surface of the china-hemp fibers after this PROCESS FOR TREATMENT smoother, remaining colloid is removed substantially, has only a small amount of fire retardant attached to fiber surface, shown in accompanying drawing 1, accompanying drawing 2 and accompanying drawing 3.
(2) for verifying the flame retardant effect of this technology, with the former flax fibre of Chinese fiber crops, come unstuck that to make length be 20cm for the back china-hemp fibers and three samples of the back china-hemp fibers of fire-retardant synchronous processings that come unstuck merely, weight is the fibre bundle of 0.3g, carries out combustion experiment, its result such as table 1 at normal temperatures and pressures:
Table 1
| Combustion characteristic | The raw ramie fibre bundle | After coming unstuck merely | After the flame treatment of coming unstuck |
| Light difficulty | Easier | Very easily | Difficult |
| Combustion characteristic | The raw ramie fibre bundle | After coming unstuck merely | After the flame treatment of coming unstuck |
| The naked light burning | Burning is very fast, and it is yellow that flame is, and the flame tail is higher, a small amount of blue smoke is arranged and burn the withered grass smell, and ashes are canescence, and hand touches friableness | It is yellow that flash fire, flame are, and the flame tail is higher, and there is a small amount of blue smoke at other position of the fiber that very easily ignites and burns the withered grass smell, and ashes are canescence, and hand touches friableness | Burning is slow, and it is yellow that flame is, and purple flame limit is arranged, and the flame tail is very low, and more hepatic cigarette is arranged, and burns the withered grass smell, and ashes are grey black |
| Force to extinguish behind the burning 2s | Fibre bundle residue 10.1cm, combustion front is more neat, black dull in saturating dark yellow | Fibre bundle residue 9.6cm, the combustion front expansion is bigger, and section is coke yellow or furvous, and ashes adhere to more | Fibre bundle residue 15.7cm, combustion front is coke black in good order |
| Required time (s) fully burnouts | 5.6 | 4.9 | 14.6 |
| After naked light extinguishes | Mars spreads about 1s | Mars spreads about 2s | Mars does not have substantially and spreads |
By data in the table as can be known, after this PROCESS FOR TREATMENT, the flame retardant effect of china-hemp fibers has also had obvious improvement.The form of three samples is shown in accompanying drawing 4, accompanying drawing 5, accompanying drawing 6 and accompanying drawing 7 behind the burning 2s.
(3) come unstuck after the fire-retardant synchronous processing the every index such as the table 2 of china-hemp fibers:
Table 2
As can be seen from Table 2, adopt this technology to come unstuck after the flame treatment, 1. lignin, pectin content and residual gum content have all had tangible reduction, especially lignin is reduced to 0.73% and 0.77% respectively after fire-retardant coming unstuck merely and come unstuck, and all is lower than 0.8%, meets the technological requirement of spinning post-finishing, residual gum content is reduced to 2.44% and 2.53% respectively, meet " process of fiber " requirement that appropriateness is come unstuck, and compare with the conventional chemical Degumming method, degumming effect is particularly evident; 2. the whiteness of fiber is greatly improved, and it is pure white smooth that fiber becomes, and is soft fine and smooth; Though 3. fiber row yielding and ultimate strength decrease, but still can guarantee the requirement of spinning post-finishing; 4. after this PROCESS FOR TREATMENT, the average diameter of fiber and average length number value diminish, and wearability makes moderate progress; 5. the limited oxygen index LOI value of fiber decreases than raw ramie after coming unstuck merely, this is because fiber disperses more, thereby easy firing more, china-hemp fibers is after the fire-retardant synchronous processing of coming unstuck, the LOI value reaches 38.9, and its flame retardant effect is greatly improved than coming unstuck merely, and after washing 20 times, still have 38.6, the wash resistant fastness of flame retardant effect is fine; 6. after the fire-retardant synchronous processing of coming unstuck, the phosphorus content of fiber reaches 1.66%, even wash 20 times, still has 1.63%, and this wash resistant fastness that flame retardant effect also is described is better; 7. the speed of these four kinds of Chinese fiber crops samples when burning is had nothing in common with each other, raw ramie contains more impurity than the Chinese fiber crops after coming unstuck merely, comprise the materials such as ash that can hinder burning, thereby its burning velocity is slow slightly, but after the fire-retardant synchronous processing of coming unstuck, its burning velocity reduces (for 2.15cm/s) greatly, it only is about 40% of raw ramie, after washing 20 times, burning velocity is still very low, this explanation fire-retardant synchronous processing of coming unstuck has greatly improved the fire resistance of fiber, and its fire-retardant persistence effect is better.
(4) this technology is merged into a step with alkali oxygen-mechanical secondary kiering and flame-proof treatment and is carried out, not only shortened flow process, saved cost, and come unstuck and flame retardant effect all be greatly improved, better than the flame-retardant after-finishing effect of carrying out at Chinese linen, the washing fastness of flame retardant effect has also had very big improvement.
(5) this technology is to be aided with quenching, heating, thermokalite bath and intensive ultraviolet radiation means on alkali oxygen-mechanically combining degumming tech basis again, and the pollutant effluents discharging is less, is a kind of relatively new technology of environmental protection.
Description of drawings
Fig. 1 is the untreated Chinese fiber crops of a present invention raw ramie SEM picture
Among the figure: the gum level of Chinese fiber crops raw ramie is higher, covers thicklyer, and covers dense evenly, and vertically is continuous band-shaped distribution along fiber.
Fig. 2 is come unstuck merely a Chinese fiber crops sem photomicrograph after handling of the present invention
Among the figure: fiber surface is smooth, does not have remaining colloid and impurity, visible many darker longitudinal grooves and part micropore.
Fig. 3 is come unstuck a Chinese fiber crops sem photomicrograph after the fire-retardant synchronous processing of the present invention
Among the figure: the fiber surface smoother, many darker longitudinal grooves are arranged, can see that also part flame-retardant composition and remaining colloid are attached to fiber surface.
Fig. 4 is the pattern (before the burning, the long 20cm of this fibre bundle, heavy 0.3g) after the former flax fibre burning of Chinese fiber crops of the present invention 2s forces to extinguish
Among the figure: raw ramie fibre bundle residue 10.1cm, dark-coloured combustion zone is darker, is about 1.2cm, because loose fiber is less, so combustion front is more concentrated, the high temperature basal seat area of coke yellow is less, is about 1cm.
Fig. 5 is the present invention's pattern (burning before, this fibre bundle long 20cm, weight 0.3g) of china-hemp fibers burning 2s after forcing to extinguish that come unstuck merely
Among the figure: fibre bundle residue 9.6cm, dark-coloured combustion zone is about 0.8cm, but owing to the flame tail in the easy burned district of loose fibres, middle part ignites, form new burning point, so the combustion front expansion is bigger, the high temperature basal seat area of coke yellow is also bigger, be about 2cm, the ashes after the burning are more.
Fig. 6 is the present invention's china-hemp fibers burning 2s of fire-retardant synchronous processing local pattern (before the burning, the long 20cm of this fibre bundle, weight 0.3g) after forcing to extinguish that comes unstuck
Among the figure: fibre bundle residue 15.7cm, the combustion zone is more shallow, and only about 0.3cm is furvous, and its combustion front does not have loose fiber substantially, and relatively more neat and concentrated, the high temperature basal seat area is about 0.7cm, is coke yellow, illustrates that its flammability is relatively poor, and flame retardant effect is relatively good.
Fig. 7 is the former flax fibre of the Chinese of the present invention fiber crops, the burning 2s of the china-hemp fibers and the fire-retardant synchronous processing china-hemp fibers that the comes unstuck pattern contrast after forcing to extinguish of coming unstuck merely
Among the figure: after three kinds of fibre bundle burning 2s force to extinguish, raw ramie residue 10.1cm, the Chinese fiber crops residue of coming unstuck merely 9.6cm, fire-retardant synchronous processing Chinese fiber crops residue 15.7cm comes unstuck, the normal combustion velocity (NCV) that can draw three kinds of Chinese fiber crops thus is respectively 4.95cm/s, 5.2cm/s and 2.15cm/s, the fire-retardant synchronous treatment process that comes unstuck has played positive effect to the fire resistance that improves china-hemp fibers.
Fig. 8 is the former flax fibre shape appearance figures of Chinese fiber crops of the present invention
Among the figure: fiber colour is dark yellow, and there are many impurity and spot in the surface, and fiber is parallel closely is arranged in many elongated sheet strips, is wound in the reunion shape each other.
Fig. 9 is a china-hemp fibers shape appearance figure after the present invention is come unstuck merely
Among the figure: fibre whiteness is significantly improved, and colloid and impurity are removed substantially, and flexibility is fine, and the fiber exquisiteness is shinny, is separated into many tuftlets and twines agglomerating each other.
Figure 10 is the present invention's fire-retardant synchronous processing back china-hemp fibers shape appearance figure that comes unstuck
Among the figure: fiber becomes pure white shinny, and the separation property between fiber and the fiber is also relatively good, and colloid and impurity are removed substantially, illustrate handle synchronously after, the degumming effect of fiber is still relatively good.
The specific embodiment
The present invention can further describe by the specific embodiment in the technical scheme described in the foregoing invention content, and its described beneficial effect also can reach its described effect by specific embodiment.
Embodiment 1
The come unstuck detailed process step of fire retardant treatment process of the former flax fibre of the Chinese of the present invention fiber crops is as follows:
One, processed by hot bath
Under 80 ℃, soak fiber 100min fully with deionized water (concentration of fiber in solution is 25g/L), and with agitator every 10min suitable/stir counterclockwise alternately it soaked evenly.Washing several times with clear water, is 7 until its soak pH value.
Two, preimpregnation acid treatment
Under 60 ℃, adopting concentration is that the dilute sulfuric acid of 9.8g/L soaks Gansu Chinese fiber crops raw ramie (concentration of fiber in solution is 25g/L) 100min fully, every 10min suitable/alternately stir counterclockwise it soaked evenly.Washing several times with clear water, is 7 until its soak pH value.
Three, pre-chlorine is handled
At normal temperatures, regulating pH value is 4, and adopting effective chlorine density is that the clorox of 1g/L soaks Gansu Chinese fiber crops raw ramie (concentration of fiber in solution is 25g/L) 40min fully, every 10min suitable/stir alternately counterclockwise that it is soaked is even.Washing several times with clear water, is 7 until its soak pH value.
Four, UV radiation
With preliminary treatment Later Han Dynasty fiber crops, put into the hydrogen peroxide of 12g/L, the NaOH of 12g/L and the magnesium sulfate mixed solution of 3.5g/L and soak (fiber is 25g/L in the concentration of solution) fully, and place radiation 40min under the ultraviolet light of wavelength 300nm, during radiation, every 10min upset once guarantees that positive and negative can both obtain radiation.
Five, quenching is freezed
Fiber and mixed solution after the taking-up radiation stir, and again it are put into plastic cup in the lump, place suddenly and freeze the freezing 240min of case, freeze fully until it.
Six, high temperature thaws
Taking-up is freezed Later Han Dynasty fiber crops and is placed 100 ℃ constant temperature boiling water to thaw fully until ice cube.
Seven, alkali oxygen-mechanical boiling-off
In the fiber after thawing, adding mixes and consoluet self-control boiling-off auxiliary agent (waterglass sodium metasilicate (Na
2SiO
3) 0.2g/L, vulcanized sodium (Na
2S) 2g/L, sodium phosphate trimer (Na
5P
3O
10) 2g/L, sodium sulfite (Na
2SO
3) 0.8g/L) stir, in 100 ℃ water bath with thermostatic control, heat 180min, and take the circumstances into consideration to add the mixed solution of a spot of NaOH, hydrogen peroxide and magnesium sulfate, to remedy the evaporation loss in the boiling-off process every 20min.During water-bath, must be 180r/min also with the agitator speed governing, every 25min suitable/stir counterclockwise alternately and make its boiling-off even.Take out fiber at last, the dilute sulfuric acid with 9.8g/L soaks 5min earlier, and cleaning until its soak pH value with clear water is 7 again.
Eight, a flame-proof treatment
1. thermokalite is bathed: the titanium pigment flame retardant, 20g/L silane resin acceptor kh-550, the 3.5g/L anion surfactant that the china-hemp fibers after the kiering are fully immersed in 160g/L
Carry out thermokalite in the mixed solution of the NaOH of H-95 and 12g/L (concentration of fiber in solution is 25g/L) and bathe processing, it is 70 ℃ that thermokalite is bathed the temperature of handling, time is 50min, carry out mechanical agitation simultaneously, stir speed (S.S.) is 90r/min, alr mode be every 20min suitable/stir counterclockwise alternately.
2. UV radiation: it is radiation 40min under the ultraviolet ray of 300nm that the china-hemp fibers after thermokalite bathed places wavelength together with mixed solution, and during radiation, every 10min upset once guarantees that positive and negative can both obtain radiation.
3. quenching is freezed: the fiber after the radiation is put into suddenly together with mixed solution and is frozen the case quenching to freezing.
Nine, secondary flame treatment
Fiber that taking-up is freezed and mixed solution repeated for the 8th step, carried out the secondary flame-proof treatment.
Ten, normal temperature unfreezing
Fiber after the secondary flame treatment and mixed solution be statically placed in the normal temperature water-bath slowly thaw.
11, scutching-dehydration-oil supply-de-oiled water-dry/dry.
Embodiment 2
According to the process of embodiment 1, the difference of embodiment 2 is:
One, when the UV radiation, hydrogen peroxide concentration is 10g/L, and naoh concentration is 10g/L, and magnesium sulfate concentration is 3g/L, and the ultraviolet radiation wavelength is 280nm, and radiated time is 30min.
Two, when the kiering of alkali oxygen, the kiering time is 150min, and the kiering temperature is 120 ℃, and agitator speed is 150r/min, alr mode be every 30min suitable/stir counterclockwise alternately.
Three, once with the secondary flame-proof treatment time, the titanium pigment flame retardant is FPK8001, and concentration is 140g/L, and silane resin acceptor kh-550 concentration is 18g/L, anion surfactant
H-95 concentration is 2g/L, and naoh concentration is 10g/L, and the thermokalite bath temperature is 60 ℃, and the time is 40min, and mechanical agitation speed is 80r/min, alr mode be every 10min suitable/stir counterclockwise alternately.The UV radiation wavelength is 280nm, and radiated time is 30min.
Embodiment 3
According to the process of embodiment 1, the difference of embodiment 3 is:
One, when the UV radiation, hydrogen peroxide concentration is 14g/L, and naoh concentration is 14g/L, and magnesium sulfate concentration is 4g/L, and the ultraviolet radiation wavelength is 350nm, and radiated time is 50min.
Two, when the kiering of alkali oxygen, the kiering time is 200min, and agitator speed is 200r/min, alr mode be every 20min suitable/stir counterclockwise alternately.
Three, once with the secondary flame-proof treatment time, the titanium pigment flame retardant is FPK8001, and concentration is 180g/L, and silane resin acceptor kh-550 concentration is 22g/L, anion surfactant
H-95 concentration is 5g/L, and naoh concentration is 14g/L, and the thermokalite bath temperature is 80 ℃, and the time is 60min, and mechanical agitation speed is 100r/min, alr mode be every 10min suitable/stir counterclockwise alternately.The UV radiation wavelength is 350nm, and radiated time is 50min.
Embodiment 4
According to the process of embodiment 1, the difference of embodiment 4 is:
One, once with the secondary flame-proof treatment time, the titanium pigment flame retardant is SAF8018, and concentration is 180g/L, and silane resin acceptor kh-550 concentration is 22g/L, anion surfactant
H-95 concentration is 5g/L, and naoh concentration is 14g/L, and the thermokalite bath temperature is 80 ℃, and the time is 60min, and mechanical agitation speed is 100r/min, alr mode be every 10min suitable/stir counterclockwise alternately.The UV radiation wavelength is 350nm, and radiated time is 50min.
Embodiment 5
According to the process of embodiment 1, the difference of embodiment 5 is:
One, once with the secondary flame-proof treatment time, the titanium pigment flame retardant is SAF8018, and concentration is 140g/L, and silane resin acceptor kh-550 concentration is 18g/L, anion surfactant
H-95 concentration is 2g/L, and naoh concentration is 10g/L, and the thermokalite bath temperature is 60 ℃, and the time is 40min, and mechanical agitation speed is 80r/min, alr mode be every 10min suitable/stir counterclockwise alternately.The UV radiation wavelength is 280nm, and radiated time is 30min.
Claims (2)
1. degumming flame-proof process technique for Han fibrilia, comprise the processed by hot bath, preimpregnation acid treatment of fiber, the process that pre-chlorine is handled, alkali oxygen-mechanically combining comes unstuck processings, thermokalite is bathed processing, quenching processing and intensive ultraviolet radiation treatment, it is characterized in that after pre-chlorine is handled, proportioning by fiber and solution is immersion 25 gram fibers in every liter of solution, and promptly the concentration of china-hemp fibers in solution is that 25g/L carries out following steps:
(1) UV radiation: will soak the china-hemp fibers of 25g/L, the hydrogen peroxide of 10-14g/L, the NaOH of 10-14g/L and the magnesium sulfate MgSO of 3-4g/L
4Mixed solution placed under the ultraviolet light of 280-350nm radiation 30-50 minute;
(2) quenching is freezed to thaw with high temperature: fiber after the radiation and mixed solution are stirred in the lump, and quenching places its taking-up 100 ℃-120 ℃ constant temperature boiling water to thaw fully until ice cube to freezing then;
(3) alkali oxygen-mechanical kiering: in the fiber after thawing, adding boiling-off additive stirs, kiering 150min-200min in 100 ℃-120 ℃ water bath with thermostatic control, and the NaOH, hydrogen peroxide and the magnesium sulfate MgSO that configure every 20min-30min adding step (1) lining
4The state of mixed solution before kiering, carry out mechanical agitation simultaneously, stir speed (S.S.) is 150-200r/min, alr mode be every 20min-30min suitable/stir counterclockwise alternately;
(4) flame-proof treatments: the titanium pigment flame retardant that 1. china-hemp fibers after the kiering is immersed in 140-180g/L is antiflaming finishing agent FPK8001 or antiflaming finishing agent SAF8018,18-22g/L silane resin acceptor kh-550,2-5g/L anion surfactant
-95 and the mixed solution of the NaOH of 10-14g/L in carry out thermokalite and bathe and handle, it is 60 ℃-80 ℃ that thermokalite is bathed the temperature of handling, and the time is 40min-60min, carries out mechanical agitation simultaneously, stir speed (S.S.) is 80-100r/min, alr mode be every 10min-20min suitable/stir counterclockwise alternately; 2. it is radiation 30min-50min under the ultraviolet ray of 280nm-350nm that the china-hemp fibers after thermokalite being bathed places wavelength together with mixed solution; 3. the fiber after the radiation is put into suddenly together with mixed solution and is frozen the case quenching to freezing;
(5) secondary flame-proof treatment: take out the fiber and the mixed solution that freeze and repeat a step;
(6) room temperature is thawed: the fiber after the secondary flame-proof treatment and mixed solution are statically placed in the room-temperature water bath slowly thaw.
2. degumming flame-proof process technique for Han fibrilia as claimed in claim 1 is characterized in that the composition of boiling-off additive and content are: waterglass sodium metasilicate (Na
2SiO
3) 0.1-0.3g/L, vulcanized sodium (Na
2S) 1-3g/L, sodium phosphate trimer (Na
5P
3O
10) 1-3g/L, sodium sulfite (Na
2SO
3) 0.7-0.9g/L.
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| CN101550653B (en) * | 2009-05-16 | 2011-05-25 | 太原理工大学 | Hemp fiber degumming boiling-off additive and preparing method thereof |
| CN101550607B (en) * | 2009-05-16 | 2011-05-25 | 太原理工大学 | Hemp fiber degumming boiling-off additive, preparing method and application thereof |
| CN102535161B (en) * | 2011-12-30 | 2013-06-26 | 太原理工大学 | Processing method for jute fabric |
| CN105463832B (en) * | 2015-03-12 | 2017-11-10 | 苏州摩维天然纤维材料有限公司 | A kind of preparation method and its flaxen fiber of the flaxen fiber with anti-flaming function |
| CN104726939A (en) * | 2015-03-19 | 2015-06-24 | 苏州陈恒织造有限公司 | Marihuana degumming process based on flash explosion-ultrasonic wave combined action |
| CN106591961B (en) * | 2016-12-13 | 2018-09-11 | 吉林大学 | A kind of flaxen fiber deep cooling-mechanically combining degumming process method |
| CN107604661A (en) * | 2017-09-29 | 2018-01-19 | 安徽省创安体育用品有限公司 | A kind of method for lifting apocynum fibre tension failure performance |
| CN109972401B (en) * | 2019-03-29 | 2021-07-20 | 西安科技大学 | Preparation method of super-amphiphobic flame-retardant high-conductivity fabric |
| CN114770838B (en) * | 2022-05-16 | 2024-10-29 | 中国科学院兰州化学物理研究所 | Preparation method of corrosion-resistant light piston for fuel tank |
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|---|---|---|---|---|
| CN1113971A (en) * | 1994-06-17 | 1995-12-27 | 山东省东平大麻纺织总厂 | Technology for quickly hemp degumming |
| CN1851062A (en) * | 2006-06-05 | 2006-10-25 | 浙江理工大学 | Hemp degumming process |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1113971A (en) * | 1994-06-17 | 1995-12-27 | 山东省东平大麻纺织总厂 | Technology for quickly hemp degumming |
| CN1851062A (en) * | 2006-06-05 | 2006-10-25 | 浙江理工大学 | Hemp degumming process |
Non-Patent Citations (1)
| Title |
|---|
| JP特开2000-128608A 2000.05.09 |
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